WO2020100714A1 - 耐炎化繊維束および炭素繊維束の製造方法ならびに耐炎化炉 - Google Patents

耐炎化繊維束および炭素繊維束の製造方法ならびに耐炎化炉 Download PDF

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Publication number
WO2020100714A1
WO2020100714A1 PCT/JP2019/043693 JP2019043693W WO2020100714A1 WO 2020100714 A1 WO2020100714 A1 WO 2020100714A1 JP 2019043693 W JP2019043693 W JP 2019043693W WO 2020100714 A1 WO2020100714 A1 WO 2020100714A1
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Prior art keywords
fiber bundle
hot air
heat treatment
treatment chamber
flame
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PCT/JP2019/043693
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English (en)
French (fr)
Japanese (ja)
Inventor
高松幸平
久慈祐介
細谷直人
山本拓
権藤和之
Original Assignee
東レ株式会社
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Application filed by 東レ株式会社 filed Critical 東レ株式会社
Priority to EP19885909.2A priority Critical patent/EP3882382A4/en
Priority to JP2019562438A priority patent/JP6729819B1/ja
Priority to US17/291,112 priority patent/US12060659B2/en
Priority to KR1020217012041A priority patent/KR20210088550A/ko
Publication of WO2020100714A1 publication Critical patent/WO2020100714A1/ja

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D01F9/225—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles from stabilised polyacrylonitriles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32—Apparatus therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32—Apparatus therefor
    • D01F9/328—Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products

Definitions

  • the present invention relates to a method for producing a flameproof fiber bundle and a carbon fiber bundle in which an acrylic fiber bundle is continuously heat-treated, and a flameproof furnace. More specifically, the present invention relates to a method for manufacturing a flameproof fiber bundle and a carbon fiber bundle, and a flameproofing furnace capable of improving the productivity and quality of the flameproof fiber bundle.
  • carbon fiber is excellent in specific strength, specific elastic modulus, heat resistance, and chemical resistance, it is useful as a reinforcing material for various materials and is used in a wide range of fields such as aerospace applications, leisure applications, and general industrial applications. Has been done.
  • a fiber bundle obtained by bundling thousands to tens of thousands of acrylic polymer single fibers is fed into a flameproof furnace and heated to 200 to 300 ° C.
  • flameproofing treatment heat treatment
  • the obtained flameproofed fiber bundle is sent to a pre-carbonization furnace and is placed in an inert gas atmosphere at 300 to 1000 ° C.
  • a method is known in which, after heat treatment (hereinafter referred to as pre-carbonization treatment) in the interior, heat treatment (hereinafter referred to as carbonization treatment) is further performed in a carbonization furnace filled with an inert gas atmosphere at 1000 ° C. or higher.
  • pre-carbonization treatment heat treatment
  • carbonization treatment heat treatment
  • the flame-resistant fiber bundle which is an intermediate material, is widely used as a material for a flame-retardant woven fabric by taking advantage of its incombustibility.
  • the heat treatment time is the longest and the amount of energy consumed is the largest in the flameproofing process. Therefore, in order to improve the productivity of the carbon fiber bundle, it is most important to improve the productivity in the flameproofing process.
  • the flameproofing process is a multi-stage horizontal heat treatment furnace in which sheet bundled fiber bundles are reciprocated in multiple stages on folding rollers arranged at both ends outside the heat treatment chamber to perform heat treatment in a heat treatment chamber in which hot air is circulated.
  • a flameproofing furnace is generally used for flameproofing.
  • the distance between the adjacent fiber bundles becomes narrower and the frequency of contact between the adjacent fiber bundles increases due to the shaking and vibration of the fiber bundles.
  • the traveling speed of the fiber bundle and to perform the heat treatment necessary for the flameproofing treatment either increase the horizontal distance between the folding rollers of the flameproofing furnace or increase the number of stages of the folding rollers, and Need to earn residence time.
  • increasing the number of stages of the folding rollers means adding a large-scale structure such as dividing the building hierarchy into a plurality of layers and increasing the load resistance of the building floor surface, which leads to a significant increase in equipment cost.
  • the horizontal distance between the folding rollers In order to increase the traveling speed of the fiber bundle while suppressing the equipment cost, it is preferable to increase the horizontal distance between the folding rollers.
  • the larger the horizontal distance between the folding rollers is the larger the hanging amount of the traveling fiber bundle becomes, and the frequency of contact between the adjacent fiber bundles increases due to the shaking / vibration of the fiber bundles as described above.
  • the mixed fibers of the fiber bundles, the breakage of the fiber bundles, and the like frequently occur, leading to deterioration of the quality of the flame-resistant fiber bundle and troubles in operation.
  • a flameproof furnace that supplies hot air in the direction parallel to the running direction of the fiber bundle is widely used.
  • the hot air blowing nozzle and the suction nozzle are vertically separated from each other, but there is no flow of hot air in the gap between the nozzles and the fiber bundle itself. Since the high-temperature hot air affected by the heat generation is accumulated, the temperature of the fiber bundle is excessively increased and the quality of the flame-resistant fiber bundle is deteriorated.
  • Patent Document 1 in order to improve heat transfer between adjacent fiber bundles while suppressing shaking / vibration of the fiber bundles, in the traveling direction of the aligned sheet-like fiber bundles, A flameproof furnace has been proposed in which the wind direction angle of hot air is defined so as to cross at an angle other than 0 ° and 90 °, preferably at an angle of 0.8 ° to 3 °.
  • Patent Document 2 in order to improve the heat transfer of the fiber bundle between the nozzles, there is proposed a flameproof furnace in which openings are provided on the upper and lower surfaces of the blowing nozzle and hot air is supplied between the nozzles.
  • the present invention is a method for producing a flameproof fiber bundle using a flameproof furnace that supplies hot air in a direction parallel to the running direction of the fiber bundle, and in a flameproof furnace, while improving the heat transfer of the fiber bundle,
  • the object is to reduce the shaking and vibration to improve the productivity and quality of the flameproof fiber bundle.
  • the manufacturing method of the flameproofing fiber bundle of the present invention has the following composition. That is, In the method for producing a flame-resistant fiber bundle, in which the aligned acrylic fiber bundles are heat-treated in a heat treatment chamber in which hot air is circulated while running on folding rollers arranged at both ends outside the heat treatment chamber, the first hot air is The fiber bundle is supplied in a direction substantially parallel to the running direction of the fiber bundle, and the second hot air is supplied from above the fiber bundle at an angle of 20 to 160 ° with respect to the wind direction of the first hot air, and the running fiber bundle Is a method for producing a flame-resistant fiber bundle, which passes at least a part in the longitudinal direction.
  • the term “substantially parallel to the running direction of the fiber bundle” in the present invention is ⁇ 0.7 with reference to the horizontal line between the vertices of a pair of opposing folding rollers arranged at both ends outside the heat treatment chamber. Refers to a direction within °.
  • the method for producing a carbon fiber bundle of the present invention has the following configuration. That is, The flame-resistant fiber bundle obtained by the above method for producing a flame-resistant fiber bundle is subjected to pre-carbonization treatment at a maximum temperature of 300 to 1000 ° C. in an inert atmosphere to obtain a pre-carbonized fiber bundle.
  • a method for producing a carbon fiber bundle which comprises carbonizing at a maximum temperature of 1000 to 2000 ° C. in an inert atmosphere.
  • the flameproofing furnace of the present invention has the following configuration. That is, A flameproof furnace for heat-treating an acrylic fiber bundle, (I) a heat treatment chamber having a slit through which the aligned fiber bundles can move in and out; (Ii) a plurality of blow-off nozzles that are arranged in the heat treatment chamber so as to be separated from each other in the vertical direction and supply the first hot air in a direction substantially parallel to the traveling direction of the fiber bundle; (Iii) a plurality of suction nozzles, which are arranged in the heat treatment chamber so as to be separated from each other in the vertical direction, and which suck the hot air supplied from the blowing nozzle, (Iv) at least one blower for circulating hot air through the blow-out nozzle and the suction nozzle, (V) at least one heating device arranged on the flow path of the circulating hot air; (Vi) A flame-proofing furnace, which is arranged outside the heat treatment chamber and includes a turn-back roller that allows the fiber bundle
  • the length of the running fiber bundle is supplied to the lower surface of the blowing nozzle from above the fiber bundle between the blowing nozzles by supplying the second hot air at an angle of 20 to 160 ° with respect to the wind direction of the first hot air.
  • a flameproofing furnace which has an opening for passing at least a part of the direction.
  • the downward wind speed of the second hot air passing through the fiber bundle is 1/3 to 5/6 of the wind speed of the first hot air flowing around the fiber bundle.
  • the downward wind speed of the second hot air passing through the fiber bundle is 1/3 to 5/6 of the wind speed of the first hot air flowing around the fiber bundle.
  • the downward air volume of the second hot air during supply is preferably 1/6 to 1/2 of the air volume of the first hot air during supply.
  • the horizontal distance between the folding rollers arranged at both ends outside the heat treatment chamber is 15 m or more.
  • the second hot air is 40 to 60% of the distance from the folding roller located at one end on the outside of the heat treatment chamber to the folding roller located at the other end. It is preferable to pass the fiber bundle at the position.
  • the opening is composed of a perforated plate, and the perforated plate has a hole diameter of 10 to 30 mm.
  • the aperture ratio of the perforated plate is preferably 20 to 60%.
  • the blowout nozzle is arranged at the center of the heat treatment chamber and the suction nozzles are arranged at both ends of the heat treatment chamber.
  • the heat transfer of the fiber bundle is improved by the second hot air, and the fiber bundle is vertically downward, which is the same direction as the suspending direction of the fiber bundle.
  • the pressing down force works to bring about the same effect as the fiber bundle is fixed at a fixed point, and it becomes possible to reduce the shaking and vibration of the fiber bundle, and as a result, the production of flame resistant fiber bundles and carbon fiber bundles. Sex and quality can be improved.
  • the flameproofing furnace of the present invention the heat transfer of the fiber bundle between the nozzles, which is most likely to be overheated by the second hot air, is improved, and the same as the suspending direction of the fiber bundle.
  • FIG. 2 is a sectional view taken along the line A-A ′ of the flameproofing furnace of FIG. 1. It is an image figure explaining contact rate P between adjacent fiber bundles. It is a schematic side surface enlarged view of the flameproofing furnace of FIG. It is a schematic side expanded view of another form of the flameproofing furnace of FIG. It is a schematic diagram of the lower surface of the blowing nozzle of FIG. It is a schematic side view of another form of the flameproofing furnace of FIG.
  • the present invention is a method of flame-proofing a fiber bundle in an oxidizing atmosphere, which is an ETE (End To End) method of circulating hot air from one end to the other end of the heat treatment chamber shown in FIG. This will be described using the flameproof furnace 1.
  • ETE End To End
  • the flameproof furnace 1 is equipped with a heat treatment chamber 3 that blows hot air onto the fiber bundles 2 traveling while folding back the multi-stage traveling area to perform flameproofing treatment.
  • the fiber bundle 2 is fed into the heat treatment chamber 3 through a slit 4 provided in the side wall of the heat treatment chamber 3 of the flameproofing furnace 1, travels linearly in the heat treatment chamber 3, and then is heat-treated through the slit 4 in the opposite side wall. It is once sent out of the room 3. After that, it is folded back by the folding rollers 5 arranged at both ends outside the heat treatment chamber 3 and fed again into the heat treatment chamber 3.
  • the fiber bundle 2 is moved in and out of the heat treatment chamber 3 a plurality of times by the plurality of folding rollers 5, and the heat treatment chamber 3 is moved in multiple stages as a whole from top to bottom in FIG. ..
  • the moving direction of the fiber bundle 2 and the number of stages of the folding roller 5 are not limited to the above.
  • the fiber bundle 2 has a wide sheet-like form in which a plurality of fiber bundles are arranged in parallel in a direction perpendicular to the paper surface as shown in FIG. While traveling inside the heat treatment chamber 3 while being folded back, the fiber bundle is subjected to flameproofing treatment with hot air at about 200 to 350 ° C. in the heat treatment chamber 3 to become a flameproof fiber bundle.
  • the hot air in the heat treatment chamber 3 is an oxidizing gas such as air and is supplied to the heat treatment chamber 3 by the blow-out nozzle 6 arranged at one end of the heat treatment chamber, and the heat treatment is performed along the traveling direction of the fiber bundle 2. It flows towards a suction nozzle 7 arranged at the other end of the chamber. Then, it is discharged from the hot air suction nozzle to the outside of the heat treatment chamber 3, guided to the hot air circulation flow path 8, heated by the heating device 9 arranged on the hot air circulation flow path 8, and the air velocity is controlled by the blower device 10. Then, the gas is again supplied from the blow-out nozzle 6 to the heat treatment chamber 3.
  • an oxidizing gas such as air
  • Such a hot-air circulation type flame-resistant furnace 1 is capable of appropriately supplying oxygen and heat to the fiber bundles 2, and repeatedly circulates the oxidizing gas heated to a high temperature, and thus has high thermal efficiency.
  • a plurality of blow-off nozzles 6 and suction nozzles 7 are provided at the upper and lower positions of the fiber bundle 2 and are vertically separated from each other in the heat treatment chamber 3.
  • the fiber bundle 2 can pass through the gap between the nozzles.
  • the pair of blowing nozzles 6 and suction nozzles 7 facing each other are arranged in a direction parallel to the traveling direction of the fiber bundle 2.
  • the running direction of the fiber bundle is, similarly to the above definition, a position where the fiber bundle separates from one of the pair of facing rollers arranged at both ends outside the heat treatment chamber and the other of the pair of facing rollers. It refers to the direction of the straight line connecting the two points of the folding roller and the position where the fiber bundle contacts.
  • the blowing nozzle 6 is provided with a resistor such as a perforated plate and a rectifying member such as a honeycomb on the blowing surface thereof so as to have a pressure loss and rectify the hot air supplied to the heat treatment chamber 3.
  • a resistor such as a perforated plate
  • a rectifying member such as a honeycomb
  • the suction nozzle 7 may be provided with a resistor such as a perforated plate on its suction surface to have a pressure loss.
  • a resistor such as a perforated plate
  • foreign matter removing means for filtering out foreign matter such as tar in the circulating hot air may be provided.
  • the foreign matter removing means is not particularly limited, but examples thereof include a wire mesh and a perforated plate such as a punching plate.
  • the hot air circulation passage 8 may be provided with a foreign matter removing means for filtering out foreign matters such as tar in the circulating hot air, if necessary.
  • the foreign matter removing means is not particularly limited, but examples thereof include a wire mesh and a perforated plate such as a punching plate.
  • an exhaust line (not shown) for exhausting a part of the circulating hot air or a supply line (not shown) for supplying clean hot air may be provided to promote the exchange of the circulating hot air in the heat treatment chamber 3. Good.
  • the heating device 9 is not particularly limited as long as it has the ability to heat hot air to a desired temperature, and for example, an electric heater or the like is used.
  • the blower device 10 is not particularly limited as long as it has desired performance, but for example, an axial fan or the like is used.
  • the “contact ratio P between adjacent fiber bundles” is used as an index.
  • the "contact rate P between adjacent fiber bundles” is the probability that the gap between adjacent fiber bundles becomes zero due to vibration in the width direction of the fiber bundles when a plurality of fiber bundles are run side by side in parallel. Refers to. In the vibration of the fiber bundle in the width direction, when the amplitude average of the fiber bundle is 0 and the standard deviation is ⁇ , the contact ratio P between adjacent fiber bundles is defined by the following equation.
  • P [1-p (x) ⁇ -t ⁇ x ⁇ t ⁇ ] ⁇ 100
  • P is the contact ratio (%) between adjacent fiber bundles
  • t is the gap (mm) between adjacent fiber bundles
  • p (x) is the probability density function of the normal distribution N (0, ⁇ 2 )
  • ⁇ is The standard deviation of the amplitude
  • x represents a random variable whose center is zero.
  • FIG. 3 is an image diagram of the contact ratio P between adjacent fiber bundles, in which the upper stage shows a plurality of traveling fiber bundles, and the lower stage shows the probability distribution of the existing positions around the right end portion of the fiber bundle at the center of the upper stage.
  • the fiber bundle vibrates, and accordingly, the gap distance t between the adjacent fiber bundles and the standard deviation ⁇ of the amplitude constantly change.
  • the distance t between the adjacent fiber bundles can be expressed by the following formula.
  • t (Wp-Wy) / 2
  • Wp is a pitch interval (mm) physically regulated by a folding roller or the like
  • Wy is a width (mm) of the running fiber bundle.
  • P corresponds to the shaded area in the lower part of FIG. 3, assuming the amplitude of the fiber bundle to be a normal distribution, and not more than the running end position of the adjacent fiber bundle (range of t when the position of the reference fiber bundle is zero)
  • the cumulative probability of / or more is P, which can be statistically calculated by actually measuring Wy and ⁇ .
  • the contact ratio P between adjacent fiber bundles is preferably 2% or more and 18% or less, and more preferably 5 to 16%.
  • the contact ratio P between the adjacent fiber bundles is within the above-mentioned preferable range, the yarn density does not become too low, and the production efficiency can be prevented from decreasing, while the mixed fiber between the adjacent fiber bundles increases.
  • the amplitude of the fiber bundle and the width of the running fiber bundle can be measured, for example, from above or below the running fiber bundle with a high-precision two-dimensional displacement sensor or the like.
  • the first hot air is supplied in a direction substantially parallel to the traveling direction of the fiber bundle 2, and at the same time, the second hot air is supplied from above the fiber bundle 2 to the first hot air. Is supplied at an angle of 20 to 160 °, and at least a part of the running fiber bundle 2 in the longitudinal direction is passed. Note that the second hot air merges with the first hot air after passing through the fiber bundle 2.
  • the flameproof furnace 1 of the present invention has a gap between the blowout nozzle 6 and the suction nozzle 7 or a heat treatment chamber 3 as shown in FIG.
  • a hot air supply device 11 for supplying the air is provided.
  • an opening 12 for supplying the second hot air is provided on the lower surface of the blowing nozzle 6.
  • the heat transfer between the nozzles having the smallest heat transfer of the fiber bundle 2 is improved, and the risk of excessive temperature rise of the fiber bundle 2 is significantly increased.
  • the blowing nozzle 6 having a positive pressure with respect to the heat treatment chamber 3 it is possible to supply the second hot air without providing an extra structure in the heat treatment chamber 3 only by providing the opening 12, so that the facility cost can be reduced. It also leads to the reduction of 4 and 5 are merely examples, and the configuration for supplying the second hot air from above the fiber bundle 2 is not limited to this.
  • the second hot air improves the heat transfer of the fiber bundle 2 as the number of supply points increases, but when the number of supply points becomes excessive, the collision between the fiber bundle 2 and the second hot air becomes excessive and the fiber bundle 2
  • the shaking and vibration of the will increase.
  • the shaking / vibration of the fiber bundle 2 is affected by the horizontal distance L between the folding rollers 5, the wind speed of the hot air circulating in the heat treatment chamber 3, and the tension of the running fiber bundle 2, but the shaking / vibration of the fiber bundle 2
  • the supply point of the second hot air is preferably 1 to 5 points, more preferably 1 to 3 points.
  • the wind direction of the second hot air is preferably 20 to 160 °, more preferably 45 to 135 ° with respect to the wind direction of the first hot air.
  • the second hot air passes between the adjacent fiber bundles 2 even if the density of the fiber bundles 2 in the heat treatment chamber 3 is increased for improving productivity. It is possible to improve the heat transfer of the fiber bundle 2. Further, since the second hot air passes between the adjacent fiber bundles 2 without increasing the wind speed, the fiber bundle 2 is effectively shaken while suppressing the collision between the fiber bundle 2 and the second hot air. Vibration can be reduced.
  • the downward air velocity passing through the fiber bundle 2 is preferably 1/3 to 5/6 of the air velocity of the first hot air flowing around the fiber bundle 2, and 1/2 to 2 It is more preferably / 3.
  • the wind speed is within the above range, the effect of downforce for pressing the fiber bundle 2 in the vertically downward direction can be sufficiently obtained while suppressing the collision of the fiber bundle 2 and the second hot air, so that the fiber bundle 2 can be effectively It is possible to reduce shaking and vibration.
  • the downward air volume of the second hot air during supply is preferably 1/6 to 1/2 of the air volume of the first hot air during supply, and more preferably 1/4 to 1/3.
  • the air volume of the first hot air at the time of supply refers to the air volume of the first hot air supplied from the blowing nozzle 6 at one location
  • the air volume of the second hot air at the time of supply is at one location.
  • the second hot air supplied from the hot air supply device 11 or the opening 12 on the lower surface of the blowing nozzle is possible to supply the second hot air satisfying the above wind speed range without disturbing the flow of the first hot air.
  • the contact area between the second hot air and the fiber bundle 2 becomes small, and the effect of down force for pressing the fiber bundle 2 in the vertically downward direction is obtained while suppressing the collision between the fiber bundle 2 and the second hot air. Therefore, it becomes possible to effectively reduce the shaking and vibration of the fiber bundle 2.
  • the horizontal distance L between the folding rollers 5 is preferably 15 m or more.
  • the staying time in the heat treatment chamber 3 is increased by 20 stages or less of the folding rollers without lowering the traveling speed of the fiber bundle 2 to less than half of the conventional speed. It becomes possible. Therefore, the equipment cost of the flameproofing furnace 1 can be reduced while maintaining the production amount of the flameproofing fiber bundle and the carbon fiber bundle per unit time, and as a result, the flameproofing fiber bundle and the carbon fiber bundle can be reduced. It is possible to improve productivity.
  • the horizontal distance L between the folding rollers 5 When the horizontal distance L between the folding rollers 5 is increased, the upstream side heat is transported to the downstream side of the circulating hot air to reach a high temperature. Therefore, the second hot air is supplied to the downstream side and the heat of the fiber bundle 2 is increased. When the transmission is improved, the excessive temperature rise of the fiber bundle 2 can be avoided, and the horizontal distance L between the folding rollers 5 can be set to 15 m or more without deteriorating the quality.
  • the second hot air passes through the fiber bundle 2 at a position of 40 to 60% of the distance from the folding roller 5 located at one end outside the heat treatment chamber 3 to the folding roller 5 located at the other end.
  • the second hot air improves the effect of fixing the fiber bundle 2 at a fixed point in the vicinity of the center of the horizontal distance L between the folding rollers 5 where the amplitude of the shaking / vibration of the fiber bundle 2 is maximized. It is possible to efficiently reduce the shaking and vibration of the.
  • the flameproofing furnace 1 of the present invention it is preferable to provide a perforated plate 13 as the opening 12 on the lower surface of the blowing nozzle 6.
  • the perforated plate 13 can provide an appropriate pressure loss to supply the second hot air uniformly rectified.
  • the hole diameter and the aperture ratio of the porous plate 13 are appropriately determined as needed.
  • the perforated plate 13 preferably has a hole diameter of 10 to 30 mm.
  • the pore diameter is within the above range, the risk that foreign matter such as tar contained in the circulating hot air is blocked by the porous plate 13 is reduced, and long-term continuous operation becomes possible.
  • the rectification of the second hot air is sufficiently performed, and the uniform second hot air is supplied in the width direction of the flameproof furnace 1, leading to the improvement of the quality of the flameproof fiber bundle. ..
  • the aperture ratio of the porous plate 13 is preferably 20 to 60% within the above range of pore diameter.
  • the second hot air can be supplied to the fiber bundle 2 without increasing the air volume, so that the fiber bundle 2 and the second hot air are effectively prevented from colliding with each other. It is possible to reduce the shaking and vibration of 2. Further, the rectification of the second hot air is sufficiently performed, and the uniform second hot air is supplied in the width direction of the flameproofing furnace 1, which leads to improvement in the quality of the flameproof fiber bundle.
  • the present invention can also be applied to a flameproof furnace having a CTE (Center To End) system configuration in which hot air is circulated from the center to both ends of the heat treatment chamber 3 shown in FIG. 7.
  • the CTE type flameproof furnace has a structure in which the blow-out nozzle 6 is arranged in the center of the heat treatment chamber 3 and the suction nozzles 7 are arranged at both ends of the heat treatment chamber 3.
  • the center of the heat treatment chamber 3 in which the blowing nozzles 6 are arranged is near the center of the horizontal distance L between the folding rollers 5, and the suspension of the fiber bundle 2 is maximized.
  • the flame-resistant fiber bundle produced by the method for producing a flame-resistant fiber bundle of the present invention is pre-carbonized at a maximum temperature of 300 to 1000 ° C. in an inert atmosphere to obtain a pre-carbonized fiber bundle.
  • a carbon fiber bundle can be manufactured by carbonizing the above at a maximum temperature of 1000 to 2000 ° C. in an inert atmosphere.
  • the maximum temperature of the inert atmosphere in the pre-carbonization treatment is preferably 550 to 800 ° C.
  • a known inert atmosphere such as nitrogen, argon or helium may be used, but nitrogen is preferable from the economical point of view.
  • the pre-carbonized fiber bundle obtained by the pre-carbonization treatment is then sent to a carbonization furnace and carbonized.
  • a carbonization furnace In order to improve the mechanical properties of the carbon fiber bundle, it is preferable to perform carbonization treatment at a maximum temperature of 1200 to 2000 ° C. in an inert atmosphere.
  • a measurement probe is inserted from a measurement hole (not shown) on the side surface of the heat treatment chamber 3 at the running position of the fiber bundle 2 immediately below the supply position, and the second hot air is blown with respect to the wind direction of the first hot air.
  • the wind velocity of the hot air flowing vertically downward was measured at five locations in the width direction.
  • the fact that a wind velocity exceeding zero is observed at all five measurement points in the width direction by the above method means that the second hot air is passing through the fiber bundle 2.
  • the measurement probe was rotated and the above measurement was performed in each wind direction, and the wind direction at which the maximum wind speed was obtained was taken as the wind direction of the second hot air.
  • a measurement probe was inserted into the blowout surface of the blowout nozzle 6 from a measurement hole (not shown) on the side surface of the heat treatment chamber 3, and the wind velocity of the first hot air was measured at five locations in the width direction.
  • the air volume of the first hot air at the time of supply was calculated from the average value and the nozzle blowing area of the blowing nozzle 6.
  • a measurement probe is inserted from a measurement hole (not shown) on the side surface of the heat treatment chamber 3 directly below the opening 12 on the lower surface of the hot air supply device 11 or the blowing nozzle, and the second hot air is directed downward.
  • the wind speed was measured at five points in the width direction, and the downward air volume of the second hot air during the supply was calculated from the average value and the supply area of the second hot air.
  • ⁇ Method of measuring yarn width and amplitude of running fiber bundle The measurement was performed at the center position between the folding rollers 5 on both sides of the flameproofing furnace 1 where the amplitude of the traveling fiber bundle was maximized. Specifically, a laser displacement meter LJ-G200 manufactured by KEYENCE CORPORATION was installed above or below the running fiber bundle and the specific fiber bundle 2 was irradiated with the laser. The distance between both ends of the fiber bundle 2 in the width direction was defined as the yarn width, and the variation in the width direction at one end in the width direction was defined as the amplitude.
  • Each of the measurements is performed once per 60 seconds or more and with an accuracy of 0.01 mm or less for 5 minutes, and the average value Wy of the width of the fiber bundle and the standard deviation ⁇ of the amplitude are acquired, and the above-mentioned “between adjacent fiber bundles” is obtained.
  • the contact rate P was calculated.
  • Tables 1 and 2 qualitatively show the results of operability, quality, and productivity in each example and comparative example. Excellent, good and bad are the following criteria.
  • the number of fluffs of 10 mm or more on the fiber bundle that can be visually confirmed after leaving the flameproofing process is an average of several fluffs / m or less, and the fluff quality is high in processability and high-order processability as a product. Level that has no effect.
  • Good The number of fluffs of 10 mm or more on the fiber bundle that can be visually confirmed after leaving the flameproofing process is 10 pieces / m or less on average, and the fluff quality is in the passability in the process and high-order processability as a product. Level that has almost no effect.
  • the number of fluffs of 10 mm or more on the fiber bundle that can be visually confirmed after leaving the flameproofing process is several tens / m or more on average, and the fluff quality is the passability in the process and the high-order processability as a product. The level that adversely affects.
  • the manufacturing cost is 80% or less of the conventional level, or the production amount per unit time is 120% or more of the conventional level.
  • Example 1 A flame-resistant fiber bundle was obtained by aligning 100 to 200 acrylic fiber bundles each consisting of 20,000 single fibers and a single fiber fineness in a sheet shape so as to be parallel to each other and heat-treating in a flame-proofing furnace 1. ..
  • the flameproof furnace 1 is a CTE system in which the horizontal distance L between the folding rollers 5 arranged at both ends outside the heat treatment chamber 3 is 20 m, the blowout nozzle 6 is arranged at the center of the heat treatment chamber 3, and the suction nozzles 7 are arranged at both ends.
  • the opening 12 was provided on the lower surface of the blowout nozzle 6 by using a perforated plate 13.
  • the openings 12 were provided at positions of 48% and 52% of the distance from the folding roller 5 located at one end on the outside of the heat treatment chamber to the folding roller 5 located at the other end, and were used for the opening 12.
  • the porous plate 13 had a hole diameter of 20 mm and an aperture ratio of 30%.
  • the wind direction of the first hot air was substantially parallel to the traveling direction of the fiber bundle 2, and the wind direction of the second hot air was 90 ° with respect to the first hot air.
  • the downward air velocity was set to 1 ⁇ 2 of the first hot air flowing around the fiber bundle 2.
  • the temperatures of the first and second hot air were 240 to 280 ° C.
  • the folding roller 5 is a groove roller provided with grooves at a predetermined interval (pitch interval to be physically regulated) Wp in the range of 3 to 15 mm.
  • the running speed of the fiber bundle 2 is adjusted in the range of 1 to 15 m / min according to the horizontal distance L between the folding rollers 5 of the flameproofing furnace 1 so that the flameproofing treatment time can be sufficiently taken, and the process tension is 0. It was adjusted in the range of 0.5 to 2.5 g / tex.
  • the flame-resistant fiber bundle obtained is then heat-treated at a maximum temperature of 700 ° C. in a pre-carbonization furnace, then heat-treated at a maximum temperature of 1400 ° C. in a carbonization furnace, and after electrolytic surface treatment, a sizing agent is applied to the carbon fiber bundle.
  • Example 2 was the same as Example 1 except that the wind direction of the second hot air was 45 ° with respect to the first hot air.
  • Example 3 Example 2 was the same as Example 1 except that the direction of the second hot air was 20 ° with respect to the first hot air.
  • Example 4 Of the second hot air passing through the fiber bundle 2 of the flameproofing furnace 1, the downward wind speed is set to 1/3 of the first hot air flowing around the fiber bundle, and the downward air volume of the second hot air at the time of supply is set.
  • Example 4 was performed in the same manner as in Example 1 except that was set to 1/6 of the air volume of the first hot air at the time of supply.
  • Example 5 Of the second hot air passing through the fiber bundle 2 of the flameproofing furnace 1, the downward wind speed is set to 5/6 of the first hot air flowing around the fiber bundle, and the downward air volume of the second hot air at the time of supply is set.
  • the air flow rate was 1 ⁇ 2 of the first hot air flow rate during the supply.
  • Example 6 Of the second hot air that passes through the fiber bundle 2, the aperture ratio of the perforated plate 13 on the lower surface of the blowout nozzle 6 of the flameproofing furnace 1 is set to 80%, and the downward wind speed of the first hot air that flows around the fiber bundle is reduced. The same procedure as in Example 1 was carried out except that it was set to 1/4.
  • Example 7 The hole diameter of the perforated plate 13 on the lower surface of the blowout nozzle 6 of the flameproofing furnace 1 is 8 mm, the opening ratio is 30%, and the downward wind speed of the second hot air passing through the fiber bundle 2 flows around the fiber bundle. Same as Example 1 except that the hot air of 1 was set to 7/8.
  • Example 8 The hole diameter of the perforated plate 13 on the lower surface of the blowout nozzle 6 of the flameproofing furnace 1 is 8 mm, the opening ratio is 30%, and the downward air volume of the second hot air at the time of supply is 1 times the air volume of the first hot air at the time of supply. Same as Example 1 except that it was set to / 8.
  • Example 9 The hole diameter of the perforated plate 13 on the lower surface of the blowing nozzle 6 of the flameproofing furnace 1 is 20 mm, the opening ratio is 80%, and the downward air volume of the second hot air at the time of supply is 3 times the air volume of the first hot air at the time of supply. Same as Example 1 except that it was set to / 5.
  • Example 10 The same procedure was performed as in Example 1 except that the horizontal distance L between the folding rollers 5 of the flameproofing furnace 1 was set to 10 m.
  • Example 11 The position of the opening 12 on the lower surface of the blowout nozzle 6 of the flameproofing furnace 1 is 35% of the distance from the folding roller 5 located at one end outside the heat treatment chamber 3 to the folding roller 5 located at the other end.
  • the same procedure as in Example 1 was performed except that it was provided at a position of 65%.
  • Example 12 The ETE method is used in which the blowout nozzle 6 is arranged at one end of the heat treatment chamber 3 of the flameproof furnace 1 and the suction nozzle 7 is arranged at the other end, and the position of the opening 12 on the lower surface of the blowout nozzle 6 is set outside the heat treatment chamber 3.
  • Example 1 was performed in the same manner as in Example 1 except that it was provided at a position of 15% of the distance from the folding roller 5 located at one end to the folding roller 5 located at the other end.
  • Example 1 was the same as Example 1 except that openings 12 were provided on the upper and lower surfaces of the blowout nozzle 6 of the flameproof furnace 1.
  • Example 1 was the same as Example 1 except that the opening 12 was provided on the upper surface of the blowout nozzle 6 of the flameproof furnace 1.
  • Example 12 was the same as Example 12 except that openings 12 were provided on the upper and lower surfaces of the blowout nozzle 6 of the flameproof furnace 1.
  • Example 12 was the same as Example 12 except that the opening 12 was provided on the upper surface of the blowout nozzle 6 of the flameproof furnace 1.
  • Example 2 was the same as Example 1 except that the direction of the second hot air was 10 ° with respect to the first hot air.
  • the present invention relates to a method for producing a flameproof fiber bundle and a carbon fiber bundle, and a flameproof furnace, which can be applied to aerospace applications, leisure applications, general industrial applications, etc., but the scope of application thereof is not limited to these. ..

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Fibers (AREA)
PCT/JP2019/043693 2018-11-12 2019-11-07 耐炎化繊維束および炭素繊維束の製造方法ならびに耐炎化炉 WO2020100714A1 (ja)

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EP19885909.2A EP3882382A4 (en) 2018-11-12 2019-11-07 METHOD FOR PRODUCING A FLAME RESISTANT FIBER BEAM AND CARBON FIBER BEAM AND FIREPROOFING FURNACE
JP2019562438A JP6729819B1 (ja) 2018-11-12 2019-11-07 耐炎化繊維束および炭素繊維束の製造方法ならびに耐炎化炉
US17/291,112 US12060659B2 (en) 2018-11-12 2019-11-07 Method of producing flame-resistant fiber bundle and carbon fiber bundle and flameproofing furnace
KR1020217012041A KR20210088550A (ko) 2018-11-12 2019-11-07 내염화 섬유다발 및 탄소 섬유다발의 제조 방법 및 내염화로

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KR20210088550A (ko) 2021-07-14
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